CN1152087C - Preparation method of wide temperature wide spectrum polyacrylic acid ester/polysiloxane composite damping rubber - Google Patents
Preparation method of wide temperature wide spectrum polyacrylic acid ester/polysiloxane composite damping rubber Download PDFInfo
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Abstract
The present invention relates to a preparation method of wide-temperature wide-spectrum polyacrylic ester/polysiloxane composite damping rubber. The preparation method is characterized in that polysiloxane and polyacrylic ester are together mixed and sulfurized, a low-temperature damping zone of the polyacrylic ester is widened, mixing rubber is used as a mother body to be interlinked with the sequence of the (methyl) polyacrylic ester, a high-temperature damping zone of composite rubber is widened, and then controllable-height and width wide-temperature wide-spectrum composite damping rubber of a polysiloxane/polyacrylic ester damping function area is prepared. The tgdelta <max> of the composite damping rubber is from 1.2 to 0.35, the temperature of the effective damping function area can reach about 250 DEG C, and the low-temperature initial transition temperature reaches -80 DEG C. The controllable-height and width wide-temperature wide-spectrum composite damping rubber can be widely applied to the aspects of shock-absorption engineering, noise-reduction engineering, etc.
Description
One, technical field
The present invention relates to a kind of preparation method of wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber, belong to functional high polymer material field.
Two, background technology
The energy that cross-linked rubber is widely used for dissipating and absorbs or contact with it is converted into heat energy with mechanical energy.But, the damping of the rubber that is made by a kind of homopolymer elastomerics usually is restricted because of the narrow glass transition region of homopolymer, because in engineering is used, often need damping rubber to have damping function in wide temperature wide frequency ranges: the damper element of the general vehicles such as train and car need have damping function in-50 ℃～+ 50 ℃ scope, aircraft, rocket require the warm territory of effective damping functional zone wideer.The effective resistance ability of damping material in wide frequency ranges is also very important, frequency as high-rise building wind resistant and anti-slight earthquake experience is 0.1～5Hz, and the damping noise reduction on naval vessel then needs the damping device external excitation of multiple frequencies such as damping ultrasonic wave and all-bottom sound simultaneously.Up to the present, technical at rubber shock-absorbing, still adopt homopolymer rubber mostly, or in the occasion that requires must have under the broad temperature, broadband effective damping function, the homopolymer rubber that has pullback capacity in differing temps (frequency) scope is bonded together, can not satisfy application requiring fully.
Polysiloxane and polyacrylic ester are two very big base polymers of polarity difference, but are considered to a pair of candidate material of performance complement always.Japan ジ エ イ エ ㄗ-Le Co., Ltd. (Japanese publication spy opens flat 10-147686) has applied for an added softening agent by siliceous polyacrylic ester preparation, can foam soft, the permanent modification of low compression, non-sticky damping rubber.This patent has been utilized the flexibility and the Abherent of polysiloxane segment well, but, owing to being added on the polyacrylic ester by the polysiloxane oligomer that has silicon hydrogen, it makes, polydimethylsiloxane oligomer molecule amount is less, and it did not embody for the effect of widening polyacrylic ester low temperature damping function district when the advantage of its high and low temperature resistance was particularly used separately.United States Patent (USP) 5,624,763 have disclosed with silicone resin and polyacrylic ester and have made pressure sensitive adhesive and coating etc., it is said that this polyacrylic ester and silicone composites have extraordinary synergistic effect, and tg δ value is high, is suitable for doing damping material especially.Though this patent has made the material in the damping function district with Gao Erkuan, but according to the tg δ-T figure that is provided, its initial transition temperature is all the time at-25 ℃ or-30 ℃, do not exceed the width that virgin pp acid esters interpenetrating polymer networks product can reach, promptly do not embody polysiloxane yet widening the contribution in polyacrylic ester damping function district.Technically, United States Patent (USP) adopts a kind of technology and photocuring technology that is situated between between blend and interpenetrating polymer networks, may be applicable to coating or thin layer of adhesive, and still, being difficult to replace with rubber is the damping element of final type of service.
Three, summary of the invention
The objective of the invention is to provide a kind of preparation method of wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber at the deficiencies in the prior art, be characterized in adopting the blend sulfurized low temperature damping district that widens polyacrylic ester of polysiloxane and polyacrylic rubber, again with blended rubber and poly-(methyl) acrylate sequence interpenetrating polymer networks, widen the high temperature damping district of compounded rubber, thereby obtain the height and the controllable broad temperature, broadband composite damping rubber of width in damping function district.
Purpose of the present invention is realized that by following technical measures raw materials used umber is parts by weight except that specified otherwise.
1. the preparation of wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber
The preparation of a, polyacrylic ester/polysiloxane blend damping rubber
With 90～10 parts of acrylate co-monomers synthetic acrylic ester copolymer rubber and/or dimethyl siloxane and acrylic ester grafted copolymer rubbers, 10～90 parts of polysiloxane, 0.5～5 part in zinc oxide, 0.5～3 part of hard ester acid, 5～10 parts of 0.5～5 part of bismaleimides and fillers, add in the mill, behind 120～25 ℃ of mixings of temperature, add 1～5 part of peroxide vulcanizing agent, in 160～170 ℃ of sulfurations of temperature 10～20 minutes, 150～175 ℃ of postcure 1～4 hour obtain polyacrylic ester/polysiloxane blend damping rubber.
The preparation of b, sequence interpenetrating polymer networks composite damping rubber
With methyl methacrylate, 100 parts of Jia Jibingxisuanyizhi and/or butyl methacrylate, 0.2～0.85 part of Diisopropyl azodicarboxylate, 1～8 part of linking agent three diglycol ethylene diacrylate, immerse by 4～40 parts of ratios in the sample of polysiloxane/polyacrylic ester vulcanized rubber, follow procedure heats up and to allow the monomer of the polymethacrylate that serves as the II network carry out polyreaction again, obtains polyacrylic ester/polysiloxane/polymethacrylate sequence interpenetrating polymer networks composite damping rubber.
The comonomer that wherein constitutes the polyacrylic ester damping rubber is a vinylformic acid 2-diethyl acetamidomalonate, butyl acrylate, propyl acrylate, ethyl propenoate, methyl acrylate and/or methacrylic ester are methyl methacrylate, Jia Jibingxisuanyizhi and/or butyl methacrylate and/or other alpha-olefin are vinylbenzene, and vinyl cyanide and/or vinyl acetate are at least a; The sulfuration monomer is 1,4 hexadiene, dicyclopentadiene and dimer thereof, and the ester derivative of ethylidene norbornene and their acrylic acid derivative or other propylene is at least a.
Wherein polysiloxane is a polydimethylsiloxane, and poly-diphenyl siloxane and/or PSI are at least a.
Wherein peroxide vulcanizing agent is 2.5-dimethyl-2.5 a di-t-butyl peroxy hexane, and dicumyl peroxide and/or di-t-butyl peroxide are at least a.
2. the preparation of polyacrylic rubber
With 60～100 parts of acrylate, 40～0 parts of methacrylic ester and/or other alpha-olefins, 3～8 parts of sulfuration monomers, 1～4 part of emulsifier sodium lauryl sulfate or Sodium dodecylbenzene sulfonate, 150～200 parts of deionized waters, oxidation-reduction initiator Sodium Persulfate-sodium bisulfite or Potassium Persulphate-ferrous sulfate, 0.01～0.4: 0.02～0.6 part, in 0～40 ℃ of reaction of temperature 4～7 hours, again with the resultant breakdown of emulsion, cohesion, dry, obtain poly-(methyl) acrylate damping rubber, owing to adopt the special molecular designing of the full method of second-order transition temperature row, the tg δ of its cross-linked rubber
MaxCan reach 1～1.2, the limited proportionality temperature increases by 20～40 ℃.
3. the preparation of siliceous polyacrylic rubber
The polydimethylsiloxane grafted acrylate rubber is carried out in two steps:
The preparation of a, polydimethylsiloxane oligopolymer
The silicone monomers that preparation polydimethylsiloxane oligopolymer is adopted is octamethylcyclotetrasiloxane (D
4), hexamethyl cyclotrisiloxane (D
3) and/or α, the oligopolymer of beta-dihydroxyl polydimethylsiloxane, comonomer are tetramethyl divinyl disiloxane or have
The monomer of structure.Wherein, X, Y, Z=-OR ,-CH
3, R=(CH
2)
n, n=1～6.With 10～98 parts of above-mentioned silicone monomers, 10～0.4 parts of comonomers, 1～5 part of Phenylsulfonic acid, 0.6～2 part of sodium lauryl sulphate or Sodium dodecylbenzene sulfonate, 150～200 parts in water, evenly blend, in 75～85 ℃ of reactions of temperature 10 hours, the acquisition molecular weight was 10～200,000 polydimethylsiloxane oligopolymer.
The preparation of b, polydimethylsiloxane graft polypropylene acid esters rubber
With 10～40 parts of polydimethylsiloxane oligopolymers, mix for 90～60 parts with acrylate, add 0.01～0.4: 0.02～0.6 part of oxidation-reduction initiator, appropriate amount of deionized water, in 0～40 ℃ of reaction of temperature 4～7 hours, product obtains polydimethylsiloxane graft polypropylene acid esters rubber through cohesion, washing, drying.This grafting elastomerics can reduce the polarity of polyacrylic ester, improves the consistency of it and polydimethylsiloxane, can be used as the expanding material of polyacrylic ester and polydimethylsiloxane, but also individual curing obtains siliceous polyacrylic rubber.
4. the preparation of PSI rubber
With α, 5～40 parts of beta-dihydroxyl methylphenyl siloxanes, 0.5～4 part in alkali glue (tetramethyl-oxyammonia 1～3%), in 90～110 ℃ of mixing of temperature, reacted 2～5 hours, vacuumize dehydration, add 95～60 parts of octamethylcyclotetrasiloxane or hexamethyl cyclotrisiloxanes, 0.03～0.07 part of 0.07～0.3 part of tetramethyl-tetrem thiazolinyl cyclotetrasiloxane and trimethylethoxysilane and/or tetramethyl divinyl disiloxane, in 90～110 ℃ of reactions of temperature 3～6 hours, the true altitude sustained reaction that progressively raises was again destroyed catalyzer after 1～6 hour, remove small molecules, obtain molecular weight and be 40～500,000 and contain the PSI rubber of different ratio phenyl.
The blended rubber sample that after above-mentioned processing, obtains, the maximum value of tg δ 1.0～1.2 low than the virgin pp acid esters on the dissipation factor curve, be generally 0.7～0.8, but, its initial transformation peaks is expanded very obvious to the low temperature direction, when blended rubber comprises 60% polydimethylsiloxane, the initial transition temperature of its second-order transition temperature transformation peaks can reach-60 ℃, 50% o'clock, reach-40 ℃, when the polydimethylsiloxane that comprises 0%, the initial transition temperature at its glass transition peak only is-19 ℃, when adopting PSI, the low temperature initial transition temperature can reach-80 ℃.
The present invention has following advantage:
1. damping material can be final type of service with vulcanized rubber or interpenetrating polymer networks product, is convenient to processing, makes the damper element of all thickness, and dimensional stability is good, good endurance.
2. rubber low temperature damping district has been widened in the adding of polysiloxane significantly.Contain 0%, 50%, 60% PDMS, the low temperature initial transition temperature of blended rubber can reach-19 ,-40 ,-60 ℃.And when containing 50%PMPS, the starting temperature of the initial transformation of blended rubber low temperature can reach-80 ℃.
3. it is narrow to have broken through blend sulfurized rubber effective damping district, often can not keep the limitation in high temperature damping district when widening the low temperature functional district.By the blend capacity increasing technique is combined with sequence interpenetrating polymer networks technology, can reach-50 ℃ at low temperature damping warm area, even-80 ℃ the time, high temperature damping function district be widened to more than 150 ℃.The leap temperature range of compounded rubber effective damping functional zone can reach 150 ℃ or 250 ℃, tg δ
MaxBe 1.2～0.35, and can adopt diverse ways, the height and the width in damping function district are controlled.
4. compounded rubber has the excellent over-all properties of polysiloxane and polyacrylic ester, with virgin pp acid esters rubber phase ratio, the water tolerance of siliceous 50% compounded rubber can improve more than 10 times, and thermotolerance obviously improves, polydimethylsiloxane and polyacrylic ester compounded rubber can improve 100 ℃ with the temperature of thermal weight loss 50% on the basis of pure acrylic acid ester, and the compounded rubber that contains methylphenyl siloxane can improve 150 ℃ with the temperature of thermal weight loss 50%.Comparing then with pure polydimethylsiloxane rubber, oil absorbency reduces by 0.5～0.7 times.In sum, compound polysiloxane/polyacrylic rubber has quite superior cost performance really, especially is suitable for doing damping material.
Four, description of drawings
Fig. 1 is the DMA figure of polymethacrylate/polydimethylsiloxane blended rubber;
Fig. 2 is the DMA figure of polyacrylic ester/polydimethylsiloxane/polymethacrylate interpenetrating polymer networks (IPN);
Fig. 3 is the DMA figure of poly-(methyl) acrylate/PSI compounded rubber.
Five, embodiment
Embodiment:
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this present embodiment can only be used for the present invention is further specified; be not understood to limiting the scope of the invention, the person skilled in the art of this area can make some nonessential improvement and adjustment to the present invention according to foregoing.
1. the preparation of wide temperature wide spectrum polyacrylic acid ester ester damping rubber
Press table 1 prescription with aforesaid propylene acid ester monomer 100g; sulfuration monomer 6.5g sodium lauryl sulphate 3g; deionized water 200g adds in the reactor; under nitrogen protection, add oxidation-reduction agent 0.03～0.2: 0.06～0.2g; reacted 5 hours down in 25 ℃ ± 2 ℃, after reaction was finished, monovalence with 2～5% or divalent salts were separated out the polyacrylic rubber cohesion; with the condensation product water rinse, obtained prepared poly-(methyl) acrylic elastomer down in dry 6～10 hours again at 60～90 ℃.
2. the preparation of siliceous poly-(methyl) acrylic elastomer
The graft copolymerization of acrylate and siloxanes is carried out in two steps: the first step is the preparation of polysiloxane oligomer.With D
4104.6g, Sodium dodecylbenzene sulfonate 1～4g, comonomer 5.0～0.4g, the pre-emulsification of water 150g, 3g mixes with Phenylsulfonic acid, reacts 10 hours down in 80～90 ℃, obtains the reactive polysiloxanes oligopolymer.
The polysiloxane oligomer that obtains diluted in proportion and add an amount of emulsifying agent; regulate PH=6; add the monomer that each prescription of 0.8 * CopII is formed; under nitrogen protection, add the former initiator of oxidation-mistake; 25 ℃ of following sustained reactions 6 hours, finish reaction after, take out the polymkeric substance that generates; cohesion, washing, drying obtain siliceous poly-(methyl) acrylic elastomer.
3. the preparation of PSI
Press ratio shown in the table 2, with the dihydroxyl methylphenyl siloxane, alkali glue 1～2.5g adds in the reactor, reacts 2 hours down in 90～110 ℃, vacuumizes and removes the water that reaction generates, and adds the D of metering
4Tetramethyl-tetrem thiazolinyl cyclotetrasiloxane 0.2g, with tetramethyl divinyl disiloxane 0.04g, add alkali glue and continue reaction 4 hours down in 90-110 ℃, sustained reaction 3～6 hours under the condition of the vacuum tightness that progressively raises again, destroy catalyzer, promptly obtain the polyphenylmethyl base silicon rubber that molecular weight 40～500,000 contain different ratio phenyl.
4. polysiloxane/polyacrylate blending rubber is with the preparation of IPN
Polyacrylic rubber (the CopI that will obtain by embodiment 1 and embodiment 2 by table 3 ratio, CopII), siliceous polyacrylic rubber (Jz) and polydimethylsiloxane (PDMS), PSI (PMPS) and zinc oxide 0.5～3g, hard ester acid 0.5～1g, bismaleimides and two 2,5 grades in two roller mills in 120～25 ℃ of uniform mixing of temperature, again in 170 ℃ of press vulcanization 10-20 minutes, 175 ℃ of postcure 4 hours promptly get blend sulfurized damping rubber.To gather (methyl) acrylate, 4%AIBN and linking agent Triethylene glycol diacrylate (TPGDA) swelling obtain PDMS/PAC rubber through sulfuration.After waiting to swell to a certain degree, again on press by 60 ℃ 2 hours, 80 ℃ 4 hours, 90 ℃ of temperature programmings in 1 hour compacting, i.e. the polysiloxane of calling sequence interpenetrating polymer networks/polyacrylic ester compounded rubber, its performance sees for details shown in table 4, the table 5.
The prescription of poly-(methyl) acrylate damping rubber of the synthetic wide temperature (wideband) of table 1
| Composition | Vinylformic acid 2-ethylhexyl (g) | Butyl acrylate (g) | Ethyl propenoate (g) | Methyl acrylate (g) | Methyl diolefinic acid methyl esters (g) | Sulfuration monomer (g) |
| CopI | 27.5 | 27.5 | 10 | 15 | 20 | 6.5 |
| CopII | 30.0 | 30.0 | 25 | 15 | / | 6.5 |
| Comparative example | / | / | 100 | / | / | 6.5 |
The prescription of table 2 preparation phenyl silicone
| The PSI of different phenyl contents | Octamethylcyclotetrasiloxane (g) | Dihydroxy-benzene radical siloxane (g) |
| High benzene | 56 | 50 |
| Middle benzene | 63 | 41 |
| Low benzene | 88 | 14 |
The processing formula of table 3 polysiloxane/polyacrylate blending rubber and IPN
| Form (wt%) | Two 2,5 (wt%) | Bismaleimides (wt%) | White carbon black (wt%) |
| CopI∶ | 1.5 | 2.0 | 10 |
| CopI∶ | 1.5 | 2.0 | 10 |
| Jz∶ | 1.5 | 2.0 | 10 |
| Constitute the monomer of IPN II network | Butyl methacrylate | Jia Jibingxisuanyizhi | Methyl methacrylate |
| Content | ～30 | ～30 | ～30 |
| TPGDA content (wt%) | 2 | 3 | 3 |
The performance of table 4 polyacrylic ester/polysiloxane blended rubber
| Tensile strength (MPa) | Elongation (%) | | 50% thermal weight loss temperature (℃) | The 24hrs water-intake rate | tgδ max * | ΔT(℃) | |
| CopI∶ | 8.08 | 360 | 35 | 350 | 1.95 | 1.21 | ～120 |
| CopI∶ | 5.95 | 280 | 32 | 500 | 0.95 | 0.64 | ～150 |
| CopI∶ | 5.35 | 240 | 32 | 450 | 0.65 | 0.70 | ～140 |
| Jz∶ | 6.42 | 280 | 34 | 400 | 1.2 | 0.60 | ～1.50 |
The performance of table 5 polyacrylic ester/polysiloxane/polymethacrylate IPN compounded rubber
| The II network is formed | Poly-n-butyl methacrylate | Polyethyl methacrylate | Polymethylmethacrylate | Poly-n-butyl methacrylate (/ polyphenylmethyl base silicon rubber) |
| Tensile strength (MPa) | 7.9 | 8.7 | 9.2 | 8.2 |
| Elongation (%) | 240 | 180 | 140 | 240 |
| tgδ max * | 0.35 | 0.45 | 0.60 | 0.59 |
| ΔT | ～115 | ～155 | ～250 | ～140 |
* (Perkindler Co.) dynamically tests on the spectrometer DMA at 7e.1 ℃/min of heat-up rate, frequency 1Hz.The thick 2mm of sample, diameter 4mm, parallel plate compact model.
Claims (7)
1, the preparation method of wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber is characterized in that:
The preparation of a, polyacrylic ester/polysiloxane blend damping rubber
With acrylate co-monomers synthetic acrylic ester copolymer rubber and/or dimethyl siloxane and acrylic ester grafted copolymer rubber 90～10 weight parts, polysiloxane 10～90 weight parts, zinc oxide 0.5～5 weight part, hard ester acid 0.5～3 weight part, bismaleimides 0.5～5 weight part and filler 5～10 weight parts, add in the mill, behind 120～25 ℃ of mixings of temperature, add peroxide vulcanizing agent 1～5 weight part, in 160～170 ℃ of sulfurations of temperature 10～20 minutes, 150～175 ℃ of postcure 1～4 hour obtain polyacrylic ester/polysiloxane blend damping rubber
The preparation of b, sequence interpenetrating polymer networks composite damping rubber
With methyl methacrylate, Jia Jibingxisuanyizhi and/or butyl methacrylate 100 weight parts, Diisopropyl azodicarboxylate 0.2～0.85 weight part, linking agent three diglycol ethylene diacrylates 1～8 weight part, immerse by 4～40 weight part ratios in the sample of polysiloxane/polyacrylic ester vulcanized rubber, follow procedure heats up and to allow the monomer of the polymethacrylate that serves as the II network carry out polyreaction again, obtains polyacrylic ester/polysiloxane/polymethacrylate sequence interpenetrating polymer networks composite damping rubber.
2, according to the preparation method of the described wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber of claim 1, wherein being used for the comonomer of synthetic polyacrylic ester damping rubber is vinylformic acid 2-diethyl acetamidomalonate, butyl acrylate, propyl acrylate, ethyl propenoate, methyl acrylate, methacrylic ester are methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate and/or other a-alkene are vinylbenzene, and vinyl cyanide and/or vinyl acetate are at least a; The sulfuration monomer is 1,4 hexadiene, dicyclopentadiene and dimer thereof, and ethylidene norbornene and their acrylate derivative thereof or other acrylate derivative are at least a.
3, according to the preparation method of the described wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber of claim 1, wherein polysiloxane is a polydimethylsiloxane, and poly-diphenyl siloxane and/or PSI are at least a.
4, according to the preparation method of the described wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber of claim 1, wherein peroxide vulcanizing agent is 2,5-dimethyl-2.5 di-t-butyl peroxy hexane; Dicumyl peroxide and/or di-t-butyl peroxide are at least a.
5, preparation method according to the described wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber of claim 1, the preparation that it is characterized in that polyacrylic rubber is with acrylate 60～100 weight parts, methacrylic ester and/or other alpha-olefin 40～0 weight parts, sulfuration monomer 1～8 weight part, emulsifier sodium lauryl sulfate or Sodium dodecylbenzene sulfonate 1～4 weight part, deionized water 150～200 weight parts, oxidation-reduction initiator Sodium Persulfate-sodium bisulfite or Potassium Persulphate-ferrous sulfate 0.01～0.4: 0.02～0.6 weight part reacted 4～7 hours down for 0～40 ℃ in temperature, again with the resultant breakdown of emulsion, cohesion, drying obtains poly-(methyl) acrylate damping rubber.
6,, it is characterized in that being prepared as of polydimethylsiloxane grafted acrylate rubber according to the preparation method of the described wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber of claim 1:
The preparation of a, polydimethylsiloxane oligopolymer
Preparation polydimethylsiloxane oligopolymer, the silicone monomers that is adopted is an octamethylcyclotetrasiloxane, hexamethyl cyclotrisiloxane and/or α, the oligopolymer of beta-dihydroxyl polydimethylsiloxane, comonomer are tetramethyl divinyl disiloxane or have
The monomer of structure, wherein, X, Y, Z=-OR ,-CH
3, R=(CH
2)
nN=1～6, with above-mentioned silicone monomers 10～98 weight parts, comonomer 10～0.4 weight parts, Phenylsulfonic acid 1～5 weight part, sodium lauryl sulphate or Sodium dodecylbenzene sulfonate 0.6～2 weight part, deionized water 150～200 weight parts, uniform mixing was in 75～85 ℃ of reactions of temperature 10 hours, the acquisition molecular weight is 10～200,000 polydimethylsiloxane oligopolymer
The preparation of b, polydimethylsiloxane graft polypropylene acid esters rubber
With polydimethylsiloxane oligopolymer 10～40 weight parts, mix with acrylate 90～60 weight parts, add oxidation-reduction initiator 0.01～0.4: 0.02～0.6 weight part, appropriate amount of deionized water, in 0～40 ℃ of reaction of temperature 4～7 hours, product obtains polydimethylsiloxane graft polypropylene acid esters rubber through cohesion, washing, drying.
7, preparation method according to the described wide temperature wide spectrum polyacrylic acid ester ester/polysiloxane composite damping rubber of claim 1, the preparation that it is characterized in that PSI is with α, beta-dihydroxyl methylphenyl siloxane 5～40 weight parts, alkali glue is 1～3% tetramethyl-oxyammonia, 0.5～4.0 weight part, in 90～110 ℃ of hybrid reactions of temperature 2～5 hours, vacuumize dehydration, add octamethylcyclotetrasiloxane or hexamethyl cyclotrisiloxane 95～60 weight parts, tetramethyl-tetrem alkene cyclotetrasiloxane 0.07～0.3 weight part and trimethylethoxysilane or tetramethyl divinyl disiloxane 0.03～0.07 weight part, in 90～110 ℃ of reactions of temperature 3～6 hours, the true altitude sustained reaction that progressively raises was again destroyed catalyzer after 1～6 hour, remove small molecules, obtain molecular weight and be 40～500,000 and contain the PSI rubber of different ratio phenyl.
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| CN100368476C (en) * | 2004-09-21 | 2008-02-13 | 广州宏昌胶粘带厂 | Preparation of wide temperature range polyacry late/polyurethane/polysiloxane damping latex |
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